Acetic Acid → 1-Methyl-6-(N-chloroacetylaminomethyl)-5-indanol

HRID 126958

반응식

HRID 126958 반응식
[CH3:1][CH:2]1[C:10]2[C:5](=[CH:6][C:7]([OH:11])=[CH:8][CH:9]=2)[CH2:4][CH2:3]1.C(O)(=O)C.S(=O)(=O)(O)O.O[CH2:22][NH:23][C:24](=[O:27])[CH2:25][Cl:26]>O>[CH3:1][CH:2]1[C:10]2[C:5](=[CH:6][C:7]([OH:11])=[C:8]([CH2:22][NH:23][C:24](=[O:27])[CH2:25][Cl:26])[CH:9]=2)[CH2:4][CH2:3]1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 62466N-Methylol-alpha-chloroacetamideHCID 893121-Methylindan-5-ol

생성물 1

HCID 202877201-Methyl-6-(N-chloroacetylaminomethyl)-5-indanol

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 850 mg of 1 methyl-5-indanol in 5 ml of a mixed solution of acetic acid and sulfuric acid (10:1 by volume) solution was mixed with 850 mg of N-hydroxymethyl chloroacetamide at room temperature under stirring for 2 hours. After reaction the reaction mixture was poured into 20 ml of water, extracted with ethyl acetate. The extract was washed with water, dried with anhydrous magnesium sulfate and concentrated under vacuum. The crude product thus obtained was purified by column chromatography on 100 g of Kiesel gel using an eluting agent comprising a mixture (20:1 by volume) of methylene chloride and ethyl acetate to provide 590 mg of the titled compound.

후처리

  1. customAfter reaction the reaction mixture
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. concentrationconcentrated under vacuum
  6. customThe crude product thus obtained
  7. customwas purified by column chromatography on 100 g of Kiesel gel

출처 및 근거

ORD 기록
ord-355a568de3424f56a7233b33c105c578
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254056

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